电感耦合等离子体质谱法测定高纯钽中21种痕量元素  

Determination of 21trace elements in high purity tantalum by ICP-MS

作　　者：吕婷 陶美娟[1,2] LüTing;Tao Meijuan(Testing Center,Shanghai Research Institution of Materials,Shanghai 200437,China;Shanghai Municipal Key Lab for Evaluation Application of Engineering Materials,Shanghai Research Institution of Materials,Shanghai 200437,China)

机构地区：[1]上海材料研究所检测中心,上海200437 [2]上海市工程材料应用与评价重点实验室,上海200437

出　　处：《分析仪器》2020年第2期48-54,共7页Analytical Instrumentation

基　　金：上海材科研究所技术创新项目(17SG-06)。

摘　　要：用硝酸-氢氟酸溶解样品,以选定的内标元素进行校正,采用电感耦合等离子体质谱法对高纯钽中21种痕量元素进行测定,按工作曲线法进行计算各元素的质量浓度,以质量分数表示测量结果。对仪器参数的优化、分析线的选择、基体干扰进行深入研究,重点考察了Sc、Y、Rh混合内标对被测元素的校正作用。结果表明:以6μg/L Rh对24Mg、27Al、50Ti、51V、52Cr、55Mn、59Co、60Ni、65Cu、66Zn、75As、90Zr、93Nb、95Mo、114Cd、118Sn、121Sb、137Ba、184W、208Pb、209Bi进行校正可以消除基体效应和信号漂移的影响。21种元素校准曲线的线性相关系数均大于0.9992,方法的检出限在0.01~0.23μg·g-1之间,测定范围为0.00 005%~0.010%。回收率在97%~105%之间,结果的相对标准偏差(RSD,n=10)小于5%。按照本方法测定高纯钽中21种痕量元素,结果与辉光放电质谱法(GD-MS)基本一致。High purity tantalum samples were dissolved by nitric acid and hydrofluoric acid,and corrected by selected internal standard elements.The working curve method was applied in calculating the mass concentration of the elements,and the test results were expressed by mass fraction.The optimization of instrumental parameters,the selection of spectral lines,and matrix effect were studied in depth.The correction effects of mixed internal standard Sc,Y,and Rh on the measured elements were investigated.The results showed that the influence of matrix effect and signal drift was eliminated when24Mg,27Al,50Ti,51V,52Cr,55Mn,59Co,60Ni,65Cu,66Zn,75As,90Zr,93Nb,95Mo,114Cd,118Sn,121Sb,137Ba,184W,208Pb and 209Bi were corrected with 6μg/L Rh.The linear correlation coefficients of calibration curves of the 21elements were all higher than 0.9992.The detection limits of the trace elements were 0.01-0.23μg·g-1,and the measurement range was 0.00 005%-0.010%.The recoveries ranged from 97.2%to105.2%,and the relative standard deviation(RSD,n=10)of the results was less than 5%.The results obtained by ICP-MS were basically consistent with those obtained by glow discharge mass spectrometry(GD-MS).

关 键 词：电感耦合等离子体质谱法(ICP-MS) 高纯钽 痕量元素 

分 类 号：TG146.416[一般工业技术—材料科学与工程] O657.63[金属学及工艺—金属材料]